CN113916996B - Column incubator for gas chromatograph and gas chromatograph - Google Patents

Column incubator for gas chromatograph and gas chromatograph Download PDF

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Publication number
CN113916996B
CN113916996B CN202010660787.XA CN202010660787A CN113916996B CN 113916996 B CN113916996 B CN 113916996B CN 202010660787 A CN202010660787 A CN 202010660787A CN 113916996 B CN113916996 B CN 113916996B
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column
sleeve
heating ring
greenhouse
heating
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CN113916996A (en
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张利军
刘懿
刘海东
胡淑娟
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Beijing Purkinje General Instrument Co Ltd
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Beijing Purkinje General Instrument Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/50Conditioning of the sorbent material or stationary liquid
    • G01N30/52Physical parameters
    • G01N30/54Temperature

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Devices For Use In Laboratory Experiments (AREA)

Abstract

The invention discloses a column temperature box for a gas chromatograph and the gas chromatograph, wherein the column temperature box comprises: the chromatographic column comprises an inner side sleeve, a heating ring and an annular centrifugal fan, wherein the heating ring is fixed in the inner side sleeve, a column greenhouse for placing the chromatographic column is formed between the heating ring and the inner side sleeve, the annular centrifugal fan is arranged in the heating ring, and a ventilation window is formed in the heating ring. The gas chromatograph has the column oven. The invention adopts the annular column greenhouse formed by the inner sleeve matched with the annular structure of the chromatographic column and the heating ring, the size of the column greenhouse can be adjusted according to the size of the chromatographic column, and the volume and the heat capacity of the column greenhouse are reduced, so that the temperature rising and falling rate of the chromatographic column is improved.

Description

Column incubator for gas chromatograph and gas chromatograph
Technical Field
The invention relates to the field of chemical analysis instruments, in particular to a column incubator for a gas chromatograph and the gas chromatograph.
Background
The structure of a conventional gas chromatograph column incubator in a laboratory is shown in fig. 1, in which a column of 30 m length is placed on a column support 103 of about 170 mm in diameter, and is placed inside a square column incubator body 101 together with a resistance wire 104 and an axial flow fan 105. When the temperature is raised, the resistance wire 104 is electrified to heat air, and the axial flow fan 105 rotates to blow hot air to the chromatographic column, so that the purpose of heating the chromatographic column is realized; when the temperature is reduced, the resistance wire 104 is powered off, the air inlet 106 and the air outlet 107 are opened, and the axial flow fan 105 rotates to replace air, so that the aim of reducing the temperature of the chromatographic column is fulfilled.
The square column incubator has the advantages of large structure volume, large heat capacity, low temperature rising and falling speed of the chromatographic column and long heating time, and can be tolerated in conventional laboratory instruments, but can not meet the requirements in applications requiring quick analysis, such as online, portable and the like.
Disclosure of Invention
The invention aims to provide a column incubator for a gas chromatograph and the gas chromatograph, which solve the problems of huge volume and low temperature rising and falling speed of the existing column incubator of the gas chromatograph.
The technical scheme of the invention is as follows:
a column incubator for a gas chromatograph, comprising: the chromatographic column comprises an inner side sleeve, a heating ring and an annular centrifugal fan, wherein the heating ring is fixed in the inner side sleeve, a column greenhouse for placing the chromatographic column is formed between the heating ring and the inner side sleeve, the annular centrifugal fan is arranged in the heating ring, and a ventilation window is formed in the heating ring. When the column temperature box is heated, the heating ring makes the temperature of the column greenhouse rise; when the column temperature box is cooled, the heating ring is closed, and the annular centrifugal fan rotates to enable the column temperature chamber to accelerate heat dissipation.
And a chromatographic column support is arranged in the column greenhouse and sleeved outside the heating ring. The chromatographic column is arranged on the chromatographic column support.
The chromatographic column support comprises at least two rings and at least two support frames, wherein the two rings are arranged at two ends of the support frames, and the support frames are used for connecting the two rings into a whole. The chromatographic column support is placed in the column greenhouse, the two rings are sleeved outside the heating ring, and the chromatographic column tray is arranged on the support frame.
The opening end of the inner sleeve is provided with an openable column greenhouse door.
The inner sleeve is provided with a ventilation window.
The column temperature box further comprises an outer sleeve, the outer sleeve is coaxial with the inner sleeve, the outer sleeve comprises two layers of cylinders, the inner sleeve is coaxial with the outer sleeve, the inner sleeve is clung to the heating ring, the outer sleeve is clung to the inner sleeve, and ventilation windows are formed in the inner sleeve and the outer sleeve. The close fit means that the distance between the inner layer cylinder and the heating ring is smaller and can be between 0 cm and 5 cm. The distance between the outer layer cylinder and the inner sleeve is the same.
The inner sleeve and the outer sleeve are relatively rotatable about a central axis.
The inner sleeve is provided with uniformly distributed ventilation windows, the inner sleeve and the outer sleeve of the outer sleeve are provided with uniformly distributed ventilation windows, and the heating ring is provided with uniformly distributed ventilation windows.
The inner sleeve and the ventilation window on the outer sleeve form an air outlet window, and the opening degrees of the air inlet window and the air outlet window are adjusted through the relative rotation of the inner sleeve and the outer sleeve.
The inner sleeve and the outer sleeve are driven by a sleeve rotating motor to rotate relatively around a central shaft.
A gear is arranged on the driving shaft of the rotating motor and is matched with a rack at the bottom of the outer sleeve to drive the outer sleeve to rotate; or the inner sleeve is driven to rotate by being matched with a rack at the bottom of the inner sleeve.
The column Wen Xiangbao comprises a temperature control system which comprises a controller and a temperature sensor, wherein the temperature sensor for measuring the temperature of the greenhouse of the column is connected with the controller and transmits temperature data to the controller, the controller is connected with the heating ring and controls the heating ring, the controller is connected with the annular centrifugal fan to control the annular centrifugal fan, and the controller is connected with the sleeve rotating motor to control the opening degrees of the air inlet window and the air outlet window.
The controller controls the heating ring, the centrifugal fan motor and the sleeve rotating motor in a PWM mode.
The heating ring is a cylinder, heating plates are fixed on the cylinder at intervals, and ventilation windows are arranged between the heating plates.
The heating sheet is a conductive ceramic heating sheet or a resistance wire heating sheet.
The invention also provides a gas chromatograph, which is provided with the column temperature box.
The beneficial effects of the invention are as follows:
an annular column greenhouse formed by an inner sleeve matched with the annular structure of the chromatographic column and a heating ring is adopted, so that the volume and the heat capacity of the column greenhouse are reduced, and the temperature rising and falling rate of the chromatographic column is improved;
adopting an annular heating mode matched with the column greenhouse annular structure to realize uniform heating of the chromatographic column and simultaneously improve the temperature rising rate;
the annular centrifugal fan heat dissipation mode matched with the column greenhouse annular structure is adopted, so that uniform heat dissipation of the chromatographic column is realized, and meanwhile, the cooling rate is improved.
The adoption and the adjustable ventilation window of column greenhouse annular structure assorted aperture has effectively promoted the homogeneity of lift temperature rate and temperature field.
Drawings
Fig. 1 is a schematic diagram of a column incubator of a gas chromatograph in the prior art.
Wherein: 101-column temperature box body, 102-column temperature box door, 103-chromatographic column support, 104-resistance wire, 105-axial fan, 106-air inlet and 107-air outlet.
Fig. 2 is a schematic structural view of a column oven according to embodiment 1 of the present invention.
Fig. 3 is a schematic structural view of a column oven according to embodiment 2 of the present invention.
Fig. 4 is an exploded view of the column oven according to embodiment 2 of the present invention.
Fig. 5 is a schematic structural view of a column support.
Fig. 6 is a schematic block diagram of the temperature control of the column oven according to embodiment 2 of the present invention.
FIG. 7 is a schematic diagram of the temperature control curve of the column oven of example 2 of the present invention.
Detailed Description
The structure and features of the present invention will be described in detail below with reference to the accompanying drawings and examples. It should be noted that various modifications can be made to the embodiments disclosed herein, and thus, the embodiments disclosed in the specification should not be taken as limiting the invention, but merely as exemplifications of embodiments, which are intended to make the features of the invention apparent.
Example 1
As shown in fig. 2, a column oven for a gas chromatograph, comprising: the chromatographic column comprises a sleeve 206, a heating ring 204 and an annular centrifugal fan 205, wherein the heating ring 204 is fixed in the sleeve 206, a column greenhouse 201 for placing the chromatographic column is formed between the heating ring 204 and the sleeve 206, and the annular centrifugal fan 205 is arranged in the heating ring 204.
The heating ring 204 comprises a cylinder 2041 and heating plates 2042, wherein the heating plates 2042 are uniformly fixed on the cylinder 2041 at intervals to form uniform annular heating, so that the chromatographic column can be rapidly and uniformly heated. The heating sheet 2042 is a conductive ceramic heating sheet or a resistance wire heating sheet. The cylinder 2041 is provided with a ventilation window 2043, and the ventilation window 2043 may be rectangular, elliptical, or a plurality of small holes or other shapes. Small vents may be provided in the sleeve 206 for heat dissipation (not shown).
The chromatographic column is wound around and fixed to a chromatographic column support 203, and the chromatographic column support 203 and the chromatographic column as a whole are placed in a column greenhouse 201.
As shown in fig. 5, the chromatographic column support 203 includes at least two rings and two supporting frames 2033, wherein one of the upper ring 2031 and the lower ring 2032 is fixedly provided with at least two supporting frames 2033 between the upper ring 2031 and the lower ring 2032, in order to make the chromatographic column support 203 more stable, four supporting frames 2033 are used in this embodiment, and the upper ring 2031 and the lower ring 2032 are fixed as a whole by the supporting frames 2033. In the embodiment, the lower circular ring is arranged as two circular rings, so that the chromatographic column can be better supported. In use, when the chromatographic column support 203 is placed in the column greenhouse 201, the chromatographic column is placed on the support 2033, and the upper circular ring 2031 and the lower circular ring 2032 are sleeved outside the heating ring 204. The number of the circular rings can be multiple, and circular rings can be additionally arranged between the upper circular ring and the lower circular ring, so that the chromatographic column support is firmer.
The sleeve 206 is provided with a column greenhouse door 202, and after the column support 203 and the column are placed in the column greenhouse 201, the column greenhouse door 202 is closed. The column greenhouse 201 may be heated by heating the heating ring 204 to increase the temperature of the column. When the temperature needs to be reduced, the annular centrifugal fan motor 207 is turned on to drive the annular centrifugal fan 205 to rotate, so that the column greenhouse 201 is reduced in temperature. Small vents in sleeve 206 also aid in heat dissipation.
The column temperature box is also provided with a temperature control system for controlling the temperature of the column temperature box, and the temperature control system is a closed-loop control system consisting of a controller, an actuator, a controlled object and a temperature sensor. Temperature data in the column temperature box are acquired through the temperature sensor and are transmitted to the controller, and the controller controls the heating ring and the annular centrifugal fan in a PWM mode according to actual conditions, so that the temperature of the column temperature box is controlled.
Example 2
As shown in fig. 3 and 4, an outer sleeve was added to the embodiment 1. The method comprises the following steps: the column Wen Xiangbao comprises two coaxially nested inner sleeves 308 and outer sleeves 309, a heating ring 304 is arranged in the inner sleeves 308, a column greenhouse 301 for placing a chromatographic column is formed between the heating ring 304 and the inner sleeves 308, an annular centrifugal fan 305 is arranged in the heating ring 304, a column greenhouse door 302 is arranged on the inner sleeves 308, a column greenhouse 301 is a cavity formed by the inner sleeves 308, the heating ring 304 and the column greenhouse door 302, and a chromatographic column support 303 and a chromatographic column are integrally placed in the column greenhouse 301.
The structure of the heating ring 304 is the same as that of the embodiment 1, and a description thereof will not be repeated.
The structure of the column holder 303 is the same as that of the column holder of example 1, and a description thereof will not be repeated.
The outer sleeve 309 comprises a two-layered barrel, with the inner barrel 3091 being coaxial with the outer barrel 3092. As shown in fig. 3, the inner tube 3091 is in close contact with the heating ring 304, the outer tube 3092 is in close contact with the inner sleeve 308, and the inner tube 3091 is provided on the side of the heating ring 304 where no heating sheet is mounted, and may be the inner side or the outer side. The outer barrel 3092 may be disposed inboard and outboard of the inboard sleeve 308. While the embodiment 2 is described in terms of the structure in which the inner tube 3091 is disposed inside the heating ring 304 and the outer tube 3092 is disposed outside the inner sleeve 308, other mounting means for the outer sleeve 309 and the inner sleeve 308 and the heating ring 304 are not shown in the drawings, but they are within the scope of the present invention.
In embodiment 2, the heating ring 304, the inner sleeve 308, the inner sleeve 3091 and the outer sleeve 3092 of the outer sleeve 309 are all provided with ventilation windows, the ventilation windows may be rectangular, elliptical, small holes, etc., and in this embodiment 2, rectangular (bar-shaped) ventilation windows are uniformly distributed, as illustrated in fig. 3, where the ventilation windows of the heating ring 304 and the inner sleeve 3091 are air inlet windows 306, and the ventilation windows of the outer sleeve 3092 and the inner sleeve 308 are air outlet windows 307.
The opening degrees of the air inlet window 306 and the air outlet window 307 are adjusted by relative rotation of the inner sleeve 308 and the outer sleeve 309.
The inner sleeve 308 and the outer sleeve 309 may be rotated relative to each other about a central axis by means of a sleeve rotating motor 311. In a specific manner, a gear 3111 is disposed on the driving shaft of the sleeve rotating motor 311, and the gear 3111 cooperates with a rack 3093 on the side of the outer sleeve 309 to drive the outer sleeve to rotate. Thereby realizing the opening and closing of the air inlet window 306 and the air outlet window 307 and the opening degree adjustment.
In this embodiment, the rack 3093 is disposed at the bottom of the outer sleeve 309, however, the rack may be disposed on the side of the inner sleeve 308, when the inner sleeve 308 is located outside the outer sleeve 309, or when the outer sleeve 309 is located outside the inner sleeve 308, the outer sleeve 309 is provided with a rack window to expose the rack on the inner sleeve 308.
The annular centrifugal fan 305 is arranged on the coaxial inner side of the annular column greenhouse 301, the annular centrifugal fan 305 rotates under the drive of the centrifugal fan motor 310, the axial air is sucked and discharged along the radial direction 360 degrees, and the axial air is sequentially discharged through the air inlet window 306 with adjustable opening, the column greenhouse 301 and the air outlet window 307 with adjustable opening, so that the rapid and uniform heat dissipation of the chromatographic column is realized in a matched mode.
Compared with the traditional column incubator, the column incubator has the advantages that the volume is reduced, the temperature rising and reducing speed is greatly improved, and the following table shows that:
traditional column incubator The column temperature box of the invention
Maximum heating rate 100 ℃/min (room temperature-400 ℃ C.) 200 ℃/min (room temperature-400 ℃ C.)
Maximum cooling rate 200 ℃/min (room temperature-400 ℃ C.) 400 ℃/min (room temperature-400 ℃ C.)
Volume (Long high thick) 300mm*300mm*350mm 128mm*124mm*190mm
As shown in FIG. 6, the invention controls the temperature of the column incubator by a temperature control system, which is a closed-loop control system composed of a controller, an actuator, a controlled object and a temperature sensor. Temperature data in the column temperature box are acquired through the temperature sensor and are transmitted to the controller, and the controller controls the opening and closing of the heating ring, the ventilation window and the centrifugal fan in a PWM mode according to actual conditions to control the temperature of the column temperature box.
As shown in fig. 7, the workflow of the temperature control system is as follows:
time t0 to t 1: the system is standby, the heating ring 304 and the annular centrifugal fan 305 stop working, the air inlet window 306 and the air outlet window 307 are closed, and the column greenhouse 301 and the chromatographic column temperature are at room temperature T0 ℃;
time t1 to time t 2: the system is started, the PID controller controls the power supply voltage of the heating ring 304 and the opening of the air inlet window 306 and the air outlet window 307 in a PWM mode, so that the temperature of the column greenhouse 301 and the chromatographic column is increased from room temperature to T1 ℃ at the heating rate of A1 ℃/min;
time t2 to time t 3: the PID controller controls the power supply voltage of the heating ring 304 and the opening of the air inlet window 306 and the air outlet window 307 in a PWM mode, so that the temperature of the column greenhouse 301 and the chromatographic column is maintained at T1 ℃;
time t3 to time t 4: the PID controller controls the power supply voltage of the heating ring 304 and the opening of the air inlet window 306 and the air outlet window 307 in a PWM mode, so that the temperature of the column greenhouse 301 and the chromatographic column is increased from T1 ℃ to T2 ℃ at the heating rate of A2 ℃/min;
time t4 to time t 5: the PID controller controls the power supply voltage of the heating ring 304 and the opening of the air inlet window 306 and the air outlet window 307 in a PWM mode, so that the temperature of the column greenhouse 301 and the chromatographic column is maintained at T2 ℃;
time t5 to t 6: the PID controller controls the power supply voltage of the centrifugal fan 305 and the opening of the air inlet window 306 and the air outlet window 307 in a PWM mode, so that the temperature of the column greenhouse 301 and the chromatographic column is reduced from T2 ℃ to T0 ℃ at the cooling rate of A3 ℃/min;
after time t 6: the system stops working and waits for the next duty cycle instruction.
The column oven of the above embodiments 1 and 2 is used in a gas chromatograph, so the present invention also provides a gas chromatograph with the column oven, and other structures in the gas chromatograph and connection relations with the column oven are all in the prior art, and are not described herein.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.

Claims (8)

1. A column oven for a gas chromatograph, comprising: the chromatographic column comprises an inner side sleeve, an outer side sleeve, a heating ring, an annular centrifugal fan and a temperature control system, wherein the heating ring is fixed in the inner side sleeve, a column greenhouse for placing the chromatographic column is formed between the heating ring and the inner side sleeve, and the annular centrifugal fan is arranged in the heating ring; the heating ring is a cylinder, and heating plates are fixed on the cylinder at intervals; a chromatographic column support is arranged in the column greenhouse and sleeved outside the heating ring;
the outer sleeve is coaxial with the inner sleeve, the outer sleeve comprises an inner layer cylinder and an outer layer cylinder, the inner layer cylinder is coaxial with the outer layer cylinder, the inner layer cylinder is clung to the heating ring, the outer layer cylinder is clung to the inner sleeve, uniformly distributed ventilation windows are formed in the inner layer cylinder and the outer layer cylinder, uniformly distributed ventilation windows are formed in the inner sleeve, and uniformly distributed ventilation windows are formed in the heating ring;
the outer sleeve and the inner sleeve are driven by a sleeve rotating motor to rotate around a central shaft relatively;
the inner sleeve and the ventilation window on the outer sleeve form an air outlet window, and the opening degrees of the air inlet window and the air outlet window are adjusted through the relative rotation of the inner sleeve and the outer sleeve;
the temperature control system comprises a controller and a temperature sensor, wherein the temperature sensor for measuring the temperature of the column greenhouse is connected with the controller and transmits temperature data to the controller;
the controller is connected with the sleeve rotating motor to control the opening degrees of the air inlet window and the air outlet window.
2. The column oven according to claim 1, wherein the chromatographic column support comprises at least two rings, at least two support frames, the two rings being disposed at both ends of the support frames, the support frames connecting the two rings together.
3. The column oven according to claim 1, wherein one end of the inner sleeve is provided with an openable and closable column greenhouse door.
4. The column incubator of claim 1, wherein a gear is arranged on the driving shaft of the sleeve rotating motor, and the gear is matched with a rack at the bottom of the outer sleeve to drive the outer sleeve to rotate; or the inner sleeve is driven to rotate by being matched with a rack at the bottom of the inner sleeve.
5. The column oven of claim 1, wherein the controller is coupled to and controls the heating ring and the controller is coupled to and controls the annular centrifugal fan.
6. The column oven of claim 5, wherein the controller controls the heating ring, the centrifugal fan motor, and the sleeve rotating motor by PWM.
7. The column oven of claim 1, wherein the heating plate is a conductive ceramic heating plate or a resistance wire heating plate.
8. A gas chromatograph having the column oven of any one of claims 1-7.
CN202010660787.XA 2020-07-10 2020-07-10 Column incubator for gas chromatograph and gas chromatograph Active CN113916996B (en)

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CN113916996B true CN113916996B (en) 2023-12-15

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101995443A (en) * 2010-09-20 2011-03-30 西华大学 Chromatograph column box
RU2529665C1 (en) * 2013-06-03 2014-09-27 Общество с ограниченной ответственностью "Научно-производственная фирма "Мета-хром" Chromatograph column thermostat
CN106706817A (en) * 2017-03-15 2017-05-24 厦门宜柱科技有限公司 Capillary liquid chromatographic column temperature control device
US9927406B1 (en) * 2017-06-02 2018-03-27 Gc Ovens Inc. Fluidless column oven for gas chromatography system
CN110664272A (en) * 2019-11-09 2020-01-10 江恩卫 Barbecue oven capable of adjusting temperature
WO2020080404A1 (en) * 2018-10-17 2020-04-23 株式会社島津製作所 Temperature control analysis device and online analysis system having temperature control analysis device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101995443A (en) * 2010-09-20 2011-03-30 西华大学 Chromatograph column box
RU2529665C1 (en) * 2013-06-03 2014-09-27 Общество с ограниченной ответственностью "Научно-производственная фирма "Мета-хром" Chromatograph column thermostat
CN106706817A (en) * 2017-03-15 2017-05-24 厦门宜柱科技有限公司 Capillary liquid chromatographic column temperature control device
US9927406B1 (en) * 2017-06-02 2018-03-27 Gc Ovens Inc. Fluidless column oven for gas chromatography system
WO2020080404A1 (en) * 2018-10-17 2020-04-23 株式会社島津製作所 Temperature control analysis device and online analysis system having temperature control analysis device
CN110664272A (en) * 2019-11-09 2020-01-10 江恩卫 Barbecue oven capable of adjusting temperature

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